CN105113247A - Coating liquid with latex particle reflection deducting capability as well as preparation method and application of coating liquid - Google Patents
Coating liquid with latex particle reflection deducting capability as well as preparation method and application of coating liquid Download PDFInfo
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Abstract
The invention discloses a coating liquid with latex particle reflection deducting capability as well as a preparation method and application of the coating liquid in a dacron fabric. The preparation method comprises the following steps: fully mixing an emulsifying agent with a part of water so as to form an emulsifying agent aqueous solution; adding a core-forming monomer and a cross-linking agent into the emulsifying agent aqueous solution, introducing protective gas so as to deoxidize for 15-20min; heating to 70-80 DEG C, adding the initiator and residual water, and reacting for 2-3 hours, so as to obtain a core-structure emulsion of latex; dropwise adding a first shell monomer and a second shell monomer into the core-structure emulsion of the latex for 1-1.5 hours; and after finishing dropwise adding, further reacting for 2-3 hours, and performing heat preservation at 85-90 DEG C for 30-45 minutes, there by obtaining the coating liquid with latex particle reflection deducting capability. The coating liquid can form a nano rough surface with low refractive index on the surface of the dacron fabric, so that reflection deduction and densification of dacron are realized, and furthermore, the structure is adhered to the fibers by virtue of shell layers and thus is endowed with a durable tidying effect.
Description
Technical field
The present invention relates to textiles auxiliary agent and preparation field thereof, be specifically related to antireflecting coating solution of a kind of emulsion particle and preparation method thereof and its application on dacron.
Background technology
Dacron have wear-resisting, stiffening, easily wash, the advantage such as quick-drying, very popular, but due to PET fiber surface level and smooth, rare reactive group and fiber (n
f=1.73) with air (n
0=1.0) between, refraction index difference is large, and incident light is reflected in a large number at fiber surface, and only fraction anaclasis enters fibrous inside, coloured light is formed after being absorbed by dye selection, therefore, cloth cover saturation degree is poor, is difficult to present the such as heavy colour effect such as blackish green, dark blue, purplish red, pitch-dark.Special when fibre number reduces, because fabric specific area increases, reflecting surface significantly increases, and make the dark problem of dye more outstanding, DYED FABRICS often presents the visual effect of one " vast expanse of whiteness ".
In conventional method, often adopt Organic fluoride, silicones Final finishing, form the smooth low-refraction antireflective resin molding of one deck at fabric face, reduce the reflectivity of cloth in the face of incident light, to increase transmitted light and to improve dyestuff color development efficiency, realize heavy colour effect.But large quantity research shows (" Anti-reflectivecoatings:Acritical; in-depthreview ", EnergyEnviron.Sci., 2011,4,3779 – 3804), this type of homogeneous antireflective coating only has higher reflection preventing ability to specific wavelength, and therefore, not only anti-reflection efficiency is low, and easily causing the change of fabric coloured light, use Organic fluoride, silicones finish fabric realize fabric increasing and are deeply restricted.
Large quantity research is separately had to show, when the nanometer coarse structure of light entrance face meets specified conditions, incident light can be caused to bending perpendicular to fabric face direction, thus form " light is caught " effect, form a kind of new anti-reflective effect, now light reflectance can be reduced to 0.1%.Based on this thought, paper " NanorougheningofPETandPTTfabricsviacontinuousUV/O3irradi ation " (DyesandPigments, 2006,69,137-143) have employed nanometer etching technology, construct stable nanometer rough surface structure, but the method depends on particular process equipment, working (machining) efficiency is low.In addition, document " Nanoporousfilmswithdesignableporositypreparedwithbinaryp olymerlatexes " (SoftMatter, 2011,7,2817 – 2824) etc. devise based on the different particle of dissolubility blended, and coated substrate surface, and then remove specified particle component in conjunction with selective solvent, obtain the method for nanometer rough surface.Although the method is ingenious, because rough surface structure depends on the initial pattern of particle, limits between particle and mutually bond, therefore membrane structure stability and the binding strength between film and base material all poor.As be applied to curvature large and the fabric fibre of flexibility increases dark time, in fabric washing and wearing process, above-mentioned nanometer coarse structure, easily by considerable damage, causes the forfeiture subtracting emitting performance.
In prior art, application number be 201210419746.7 patent of invention disclose a kind of copolymer emulsion type dacron deep-dyeing agent and preparation method thereof, auxiliary agent be mainly used in dacron increase deep processing.Auxiliary agent is based on organic sesqui siloxane and epoxy chlorine alkane modified amino silicon oil is composite, prepared by copolymerization.In addition, prior art application number be 201310713917.1 patent of invention disclose a kind of preparation method of environment-friendlytype type fabric deep-dyeing agent, this technology is done mainly for dacron and is increased depths reason, have employed organic silicon monomer in invention, fluorochemical monomer carries out modification to acrylate copolymer, generate the deep-dyeing agent of organosilicon (/ fluorine)-acrylic ester copolymer structure, and employing is padded and soaking technology increases dark finish fabric.When adopting this two kinds of methods, although finish fabric obtains increase dark effect, in patent, not mentioned auxiliary agent is at the pattern of finish fabric surface construction, also has no the description increasing dark fabric based on " nanometer rough surface ".
Chinese patent ZL201210303496.0 proposes with polymer coated silica, and bakes film forming based on sheath polymers, silica is adhered to fabric face, constructs the method for nanometer coarse structure.Afterwards, in application number 201410412286.4 Chinese patent application, propose a kind of based on polyster fibre plasticizing bonding silica, construct the method for antireflective rough surface.In two kinds of methods, coarse structure largely depends on silica particle diameter.
Compare silica, the particle diameter of emulsion particle can regulate conveniently by emulsifier concentration and kind, and modulation process is ripe.Therefore, if realize constructing fabric face coarse structure based on emulsion particle, be not only convenient to surface roughness, and by selecting monomer, also can reduce the refractive index of rough surface further.
Summary of the invention
The invention provides antireflecting coating solution of a kind of emulsion particle and preparation method thereof and its application on dacron, this coating solution can form low-refraction nanometer rough surface on dacron surface, realize terylene antireflective and increase dark.
A preparation method for the antireflecting coating solution of emulsion particle, comprises the following steps:
(1) " core-shell structure copolymer " latex kernel preparation: fully stirred by the water of emulsifying agent and partial amount, forms emulsifier aqueous solution, is added in emulsifier aqueous solution by nuclear monomer processed, crosslinking agent, and logical protective gas is (as N
2) deoxygenation 15 ~ 20min, when being warming up to 70 DEG C ~ 80 DEG C, add the water of initator and surplus, after reaction 2 ~ 3h, obtain the nuclear structure emulsion of latex;
(2) " core-shell structure copolymer " structure is formed: in the nuclear structure emulsion of latex, drip the first shell monomer and the second shell monomer, time for adding is 1 ~ 1.5h, after dropping terminates, after continuing reaction 2 ~ 3h, at 85 DEG C ~ 90 DEG C insulation 30 ~ 45min, obtain the antireflecting coating solution of emulsion particle, namely there is " core-shell structure copolymer " latex aqueous dispersions of crosslinked kernel.
The present invention has cross linked chain structural polymer kernel by preparation, and " core-shell structure copolymer " emulsion particle of linear flexible polymer shell, and by the temperature adjusting in arrangement process, induce shell interpolymer chain phase counterdiffusion in adjacent emulsion particle, by bonding for adjacent emulsion particle kernel, and with the high fastness of fiber surface sticky and.Of particular note, due in said process, kernel is highly cross-linked, the diffusion of kernel polymer chain is suppressed, and therefore, kernel is difficult to cave in, in glued membrane, keep initial nanometer spherical-like morphology, thus give the stabilized nanoscale coarse structure on latex film and then finish fabric surface.Because shell is formed containing alkene double bond organic silicon monomer and acrylate monomer copolymerization with low-refraction, therefore film surface has low-refraction attribute.Thus, this structure can produce " light is caught " effect, avoids the dependence of antireflective to wavelength, and the change to fabric coloured light.In the method, because latex particle size is easily adjusted, its coarse structure formed is easy to customization.And this structure, by shell bondable fibers, gives finishing effect durability.
As preferably, aforesaid operations step, with parts by weight, adopts the raw material of following weight portion:
Further preferably, with parts by weight, the raw material of following weight portion is adopted:
In step (1), as preferably, described nuclear monomer processed is methyl methacrylate.Polymethyl methacrylate has lower refractive index (n=1.41), superior good heat resistance, light transmittance is high, dispersion is little and rigidity, forms the nanosphere form of latex film as emulsion particle inner core structure.
As preferably, described crosslinking agent is the one in divinylbenzene, Ethylene glycol dimethacrylate.Crosslinking agent can increase the cohesive strength of core-shell particles in toughening modifying, and makes kernel be limited to cross-linked structure, is difficult to cave in, and keeps the initial nanosphere form of inner core structure, to realize the stable nanometer coarse structure of latex film.
As preferably, described emulsifying agent is the one in lauryl sodium sulfate, sodium soap, sodium alkyl sulfonate, neopelex.Anionic emulsifier can give core-shell latex particles surface charge, efficient stable latex.And nonionic emulsifier can strengthen latex electrolyte-resistant ability, improve the compatibility increasing dark auxiliary agent and other saliferous finishing auxiliarieses.
As preferably, described initator is the one in potassium peroxydisulfate, ammonium persulfate.Initator add the form that can adopt initiator solution.
In step (2), as preferably, the first described shell monomer is one or both in butyl acrylate, acrylonitrile.As linear flexible polymer shell structurre, by the temperature adjusting in arrangement process, can lure shell interpolymer chain phase counterdiffusion in adjacent emulsion particle into, form the latex film with continuous structure, the height between realization and fabric glues and fastness.
As preferably, the second described shell monomer is one or both in methacryloxypropyl trimethoxy silane, [4-(methacryloxypropyl) butyl] pentamethyl siloxanes.
The solid content of the antireflecting coating solution of emulsion particle prepared by preparation method of the present invention (namely having " core-shell structure copolymer " latex aqueous dispersions of crosslinked kernel) is 10% ~ 30%, preferred latex particle size is 50nm ~ 150nm, and nucleocapsid mass ratio is 7:3 ~ 9:1.
What preparation method of the present invention obtained has cross-linked polymer chain structure kernel, and " core-shell structure copolymer " emulsion particle aqueous dispersion coating solution of linear flexible polymer shell, the i.e. antireflecting coating solution of emulsion particle, can be used as structure dacron nano surface coarse structure, realizes fabric and increase dark.When this coating solution arranges deeply for dacron increasing, the technique for applying adopted specifically comprises: join in the water of 90 ~ 99 weight portions by 1 ~ 10 weight portion emulsion particle antireflection coatings liquid, forms emulsus dressing liquid.Adopt padding method to arrange fabric afterwards, after baking, obtain the dacron after arranging.
As preferably, described padding method is that method is rolled in two leachings two, and pick-up rate is 30% ~ 70%.
As preferably, train baking condition: baking temperature is 150 DEG C ~ 170 DEG C, and the time is 60s ~ 100s.
Compared with prior art, tool of the present invention has the following advantages:
The invention provides antireflecting coating solution of a kind of emulsion particle and preparation method thereof and its application on dacron, this coating solution has cross-linked polymer chain structure kernel by one, and " core-shell structure copolymer " emulsion particle dispersion liquid composition of linear flexible polymer shell, low-refraction nanometer rough surface can be formed on dacron surface, realizing terylene antireflective increases dark, and its advantage is:
(1) based on sheath polymers bonding, the nanometer coarse structure formed at fabric face is stablized;
(2) regulated and controled by synthesis process, conveniently adjusted latex particle size and " core-shell structure copolymer " ratio, and then customize its nanometer coarse structure formed at fabric face;
(3) coating solution preparation feedback is medium with water, avoids with an organic solvent, arranges the release of process organic solvent-free;
(4) finishing technique is simple.
Prepared emulsion particle antireflection coatings liquid, can directly be coated in dacron surface, bake in film forming procedure, shell interpolymer chain phase counterdiffusion in adjacent emulsion particle, forms the latex film with continuous structure.In the process, kernel is limited to cross-linked structure, is difficult to cave in, and keeps initial nanosphere form, and gives latex film stable nanometer coarse structure, at the antireflective coating that dacron surface construction is stable.Because shell is formed containing alkene double bond organic silicon monomer and acrylate monomer copolymerization with low-refraction, therefore film surface has low-refraction attribute.Incident light is after in film, multiple solutions place is reflected, bending to perpendicular to fabric face direction, forms " light is caught " effect, realizes antireflective and increase dark effect.
Accompanying drawing explanation
Fig. 1 is the grain size distribution of the emulsion particle product 1 obtained in the embodiment of the present invention 1;
Fig. 2 is the photo of the transmission electron microscope (TEM) of the emulsion particle product 1 obtained in the embodiment of the present invention 1;
Fig. 3 is that AFM (AFM) figure of product 1 latex film in the embodiment of the present invention 1 represents;
Fig. 4 is the photo of the transmission electron microscope (TEM) of the emulsion particle product 2 obtained in the embodiment of the present invention 2;
Fig. 5 is that AFM (AFM) figure of product 3 latex film in the embodiment of the present invention 3 represents;
Fig. 6 is ESEM (SEM) figure of dacron surface topography before application examples 1 floating coat liquid of the present invention arranges;
Fig. 7 is ESEM (SEM) figure of the dacron surface topography that comparative example product 4 of the present invention arranges;
Fig. 8 is ESEM (SEM) figure of the dacron surface topography after the product 2 obtained in the embodiment of the present invention 2 arranges.
Fig. 9 is that the dacron apparent shade depth value that arranges of product 2 of the present invention arranges the change curve with wavelength at temperature in difference.
Figure 10 is that product 1 of the present invention, product 2, product 3 and product 4 arrange the change curve of dacron apparent shade depth value with wavelength.
Detailed description of the invention
Embodiment 1
The lauryl sodium sulfate taking 0.2g joins in the water of 74.77g, after mechanical agitation mixes, adds the methyl methacrylate of 10g and the divinylbenzene of 8g in solution, after mechanical agitation is even, puts into the logical N of water-bath
215min, after being warming up to 75 DEG C, 0.03g potassium peroxydisulfate to be dissolved in 5g water and to join in above-mentioned reaction mixture, after reaction 2.5h, obtain reactant liquor (i.e. the nuclear structure emulsion of latex), in reactant liquor, slowly drip the mixed liquor of 1.5g butyl acrylate and 0.5g methacryloxypropyl trimethoxy silane, drip in 0.5h.After continuing reaction 3h, be warming up to 90 DEG C and be incubated 30min, the antireflection coatings liquid that the obtained emulsion particle solution product 1 with nucleocapsid structure forms, solid content is 20%.
Product 1 is carried out dilute rear employing Malvern nanometer particle size instrument and measure its grading curve respectively, as shown in Figure 1, the particle diameter of product 1 is at about 85nm, and domain size distribution is stablized.
By particle after osmic acid dyeing, observe with transmission electron microscope (TEM), as shown in Figure 2.
After product 1 is coated with the latex film made, observe with AFM (AFM), as shown in Figure 3.
Embodiment 2
The neopelex taking 0.5g joins in the water of 67.46g, after mechanical agitation mixes, adds the methyl methacrylate of 12g and the Ethylene glycol dimethacrylate of 8g in solution, after mechanical agitation is even, puts into the logical N of water-bath
220min, reach after to 70 DEG C until temperature, 0.04g potassium peroxydisulfate to be dissolved in 5g water and to add in above-mentioned reaction mixture, after reaction 2h, in reactant liquor, slowly drip the mixed liquor of 5g butyl acrylate and 2g methacryloxypropyl trimethoxy silane, drip in 2h.After continuing reaction 2.5h, be warming up to 85 DEG C and be incubated 45min, the antireflection coatings liquid that the obtained emulsion particle solution product 2 with nucleocapsid structure forms, solid content is 27%.
Fig. 4 is the TEM photo of product 2.As can be seen from Figure 4, product 2 defines nucleocapsid structure, still maintains good dispersity, even particle size, substantially exists with primary particle form.
Embodiment 3
The sodium alkyl sulfonate taking 1g joins in the water of 68.95g, after mechanical agitation mixes, adds the methyl methacrylate of 10g and the divinylbenzene of 5g in solution, after mechanical agitation is even, puts into the logical N of water-bath
220min, reach until temperature and after to 80 DEG C, 0.05g ammonium persulfate to be dissolved in 5g water and to add in above-mentioned reaction mixture, after reaction 3h, in reactant liquor, slowly drip the mixed liquor of 8g acrylonitrile and 2g [4-(methacryloxypropyl) butyl] pentamethyl siloxanes, drip in 2h.After continuing reaction 3h, be warming up to 90 DEG C and be incubated 40min, the antireflection coatings liquid that the obtained emulsion particle solution product 3 with nucleocapsid structure forms, solid content is 25%.
Fig. 5 is the AFM photo of product 3 latex film, and visible film coated surface has concavo-convex nanometer coarse structure.From Fig. 3 and Fig. 5, product 3 the varying in size of nano particle compared with product 1, but its pattern is without significant difference, still maintains good dispersity, even particle size, substantially exists with primary particle form.
Comparative example:
The sodium soap taking 0.2g joins in the water of 84.77g, after mechanical agitation mixes, the mixed liquor of the methyl methacrylate of 6g, the Ethylene glycol dimethacrylate of 2.5g, 1g divinylbenzene and 0.5g [4-(methacryloxypropyl) butyl] pentamethyl siloxanes is added in solution, after mechanical agitation is even, put into the logical N of water-bath
220min, reach until temperature and after to 75 DEG C, the potassium peroxydisulfate of 0.03g to be dissolved in 5g water and to join in above-mentioned reaction mixture, after continuing reaction 2.5h, be warming up to 90 DEG C and be incubated 35min, the antireflection coatings liquid of obtained homogenized milk particle solution product 4 composition, solid content is 10%.
Application examples 1 (adopting product in embodiment 1):
Take the emulsion particle coating solution in 1.5g embodiment 1, be dissolved in the water and be mixed with the solution of 30mL.First immersed by dacron in emulsus dressing liquid, adopt two leachings two method of rolling to arrange dacron, pick-up rate is 65%.60s is dried, the dacron after finally being arranged 170 DEG C of trainings.
Application examples 2 (adopting product in embodiment 2):
Take the emulsion particle coating solution in 0.9g embodiment 2, be dissolved in the water and be mixed with the emulsus dressing liquid of 30mL.First immersed by dacron in emulsion particle dressing liquid, adopt two leachings two method of rolling to arrange dacron, pick-up rate is 60%.90s is baked, the dacron after finally being arranged at 165 DEG C.
Take identical method for sorting, be mixed with emulsus dressing liquid with comparative example product 4 and arrange dacron as a comparison case, observe the surface topography of polyster fibre with scanning electronic microscope (SEM).Fig. 6 is former dacron surface topography map.Fig. 7 is the dacron surface topography map that the product 2 obtained in embodiment 2 arranges.Fig. 8 is the dacron surface topography map that comparative example product 4 arranges.Comparison diagram 6, Fig. 7 and Fig. 8, find that the PET fiber surface after product 2 and product 4 arrange all is coated with and be covered with emulsion particle coating.After product 2 arranges, dacron surface forms nanometer coarse structure.And after adopting comparative example product 4 to arrange, dacron surface is still smooth.Can expect that product 2 coated film has the reflection preventing ability being better than product 4 coated film.
Meanwhile, for investigating the Film Morphology of latex film in PET fiber surface, baking of different temperatures being carried out to the dacron that product 2 emulsus finishing agent in embodiment 2 arranges, characterizing its apparent dark value change with color measurement and color match instrument SF600-PLUS.With unfinished dacron as a comparison.Fig. 9 is dacron apparent shade depth value curve with the change of wavelength under difference arranges temperature.
Contrast application examples (adopting product in comparative example)
Take the emulsion particle coating solution of product 4 in 2.25g comparative example, be dissolved in the water and be mixed with the solution of 30mL.First immersed by dacron in emulsus dressing liquid, adopt two leachings two method of rolling to arrange dacron, pick-up rate is 70%.Dry 100s 160 DEG C of trainings, obtain the dacron after product 4 coating solution arranges.
The apparent shade depth value of dacron after product 1, product 2, product 3 and product 4 coating solution arrange is characterized respectively with color measurement and color match instrument SF600-PLUS.Figure 10 is that four kinds of products arrange the change curve of dacron apparent shade depth value with wavelength.
Claims (10)
1. a preparation method for the antireflecting coating solution of emulsion particle, is characterized in that, comprise the following steps:
(1) water of emulsifying agent and partial amount is fully stirred, form emulsifier aqueous solution, nuclear monomer processed, crosslinking agent are added in emulsifier aqueous solution, logical protective gas deoxygenation 15 ~ 20min, when being warming up to 70 DEG C ~ 80 DEG C, add the water of initator and surplus, after reaction 2 ~ 3h, obtain the nuclear structure emulsion of latex;
(2) in the nuclear structure emulsion of latex, drip the first shell monomer and the second shell monomer, time for adding is 1 ~ 1.5h, drips after terminating, and after continuing reaction 2 ~ 3h, at 85 DEG C ~ 90 DEG C insulation 30 ~ 45min, obtains the antireflecting coating solution of emulsion particle.
2. the preparation method of the antireflecting coating solution of emulsion particle according to claim 1, is characterized in that, with parts by weight, adopts the raw material of following weight portion:
3. the preparation method of the antireflecting coating solution of emulsion particle according to claim 2, is characterized in that, with parts by weight, adopts the raw material of following weight portion:
4. the preparation method of the antireflecting coating solution of emulsion particle according to claim 1, is characterized in that, in step (1), described nuclear monomer processed is methyl methacrylate.
5. the preparation method of the antireflecting coating solution of emulsion particle according to claim 1, is characterized in that, in step (1), described crosslinking agent is the one in divinylbenzene, Ethylene glycol dimethacrylate.
6. the preparation method of the antireflecting coating solution of emulsion particle according to claim 1, it is characterized in that, in step (1), described emulsifying agent is the one in lauryl sodium sulfate, sodium soap, sodium alkyl sulfonate, neopelex.
7. the preparation method of the antireflecting coating solution of emulsion particle according to claim 1, is characterized in that, in step (1), described initator is the one in potassium peroxydisulfate, ammonium persulfate.
8. the preparation method of the antireflecting coating solution of emulsion particle according to claim 1, is characterized in that, in step (2), the first described shell monomer is one or both in butyl acrylate, acrylonitrile;
The second described shell monomer is one or both in methacryloxypropyl trimethoxy silane, [4-(methacryloxypropyl) butyl] pentamethyl siloxanes.
9. according to the antireflecting coating solution of emulsion particle prepared by the arbitrary described preparation method of claim 1 ~ 8.
10. the antireflecting coating solution of emulsion particle according to claim 9 increases the application in dark arrangement at dacron.
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Application publication date: 20151202 Assignee: Zhejiang Sci-Tech University Shangyu Industrial Technology Research Institute Co., Ltd. Assignor: Zhejiang University of Technology Contract record no.: X2019330000038 Denomination of invention: Coating liquid with latex particle reflection deducting capability as well as preparation method and application of coating liquid Granted publication date: 20170707 License type: Common License Record date: 20191108 |